Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Novel Water Cluster [Mn(phen)_2·H_2O·Cl]·p-FBA·3H_2O

A novel water cluster [Mn(phen)2·H2O·Cl]·p-FBA·3H2O (p-FBA = p-fluorobenzoic acid and phen = 1,10-phenanthroline) was synthesized by the hydrothermal reaction of MnCl2 with p-FBA and phen at 150 ℃ and characterized by elemental analysis,IR spectra and TG. Its crystal structure was determined by X-ray single-crystal diffraction study. The crystal belongs to the triclinic system,space group P1,with a = 10.5768(1),b = 11.5960(1),c = 12.9916(2) ,α = 101.816(2),β = 95.397(2),γ = 103.052(2)o,V = 1502.8(3) 3,Z = 2,Dc = 1.463 g/cm3,R = 0.0399 and wR = 0.0997. The crystal structure shows that the manganese(Ⅱ ) ion is six-coordinated by four nitrogen atoms,one chloride ion and one oxygen atom forming a distorted octahedral coordination geometry. The structure includes three acyclically connected water molecules and one coordinated water molecule thus forming a (H2O)4 water cluster. This water pattern forms a cross-linked discrete ring. The steady (H2O)4 is further extended into a cage-like structure by the hydrogen-bonding interaction formed by dissociative aqua molecule and Cl-ligand. The dimer structure is further extended into a one-dimensional (1D) structure through C-H···O interaction. π···π Stacking interaction among adjacent phen aromatic rings further stabilizes the crystal structure.     

Crystal Structure and Conformation of [1-(β-D-lyxofuranosyl)uracil]- 2''''-spiro-5"-[4"-(S)-(diethoxyphosphinyl)-2"-oxazoline]

1 INTRODUCTION It is well known that natural and modified nucleosides have potential antiviral and anticancer activities[1,2]. These observations prompted us to synthesize the title compound －a new kind of spironucleoside, whose structure was determined by 1HNMR, 31PNMR and elemental analysis. The configuration was assigned by means of nuclear Overhauser effect. To further confirm the structure and configuration unambiguously, the title compound was subjected to X-ray diffractio…     

Synthesis, Structure and Properties of (n-Bu_4N)_3[Mo_6O_18NNAr(NO_2)_2]

The title compound was synthesized and characterized by means of elemental analysis, IR, DTA-TG and UV. Its single crystal structure was solved by using direct methods. The compound crystallizes in the orthorhombic space group Pmc(?) with lattice parameters: a = 1. 7261(2), b=l. 7537(3), c=2. 4258(3) nm. V=7. 34220 nm3, F(000) = 3648, Z = 4. The structure was refined to conventional discrepancy factors of R=0. 060 for 3176 observed reflections [Ⅰ>3σ/(Ⅰ)]. The anion represents a modification of the well-known [Mo6O19]2- anion, in which a single terminal oxo group is replaced by a 2,4-dinitrophenyl hydrazine ligand while the structure integrity of the hexanuclear framework is maintained.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]~(2 )·[SbCl_5]~(2-)}_2

A new supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2,was synthesized by the hydrothermal reaction of o-diaminobenzene,2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution,and characterized by chemical analysis,elemental analysis,IR spectra,thermogravimetric analysis and fluorescence spectra. The crystal structure was deter-mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system,space group P21/c,with a=16.0397(13),b=14.3189(12),c=15.6370(13),β=105.8980(10)°,V=3454.0(5)3,Z=4,C24H22Cl10N6Sb2,Mr=992.48,Dc=1.909 g/cm3,μ=2.366 mm-1,S=1.010,F(000)=1920,R=0.0254 and wR=0.0555. The coordination anion,[SbCl5]2-which is a distorted tetragonal pyramid,is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2-form a biquaternion ring structure through the secondary bonding of Sb···Cl. Moreover,the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridyl)benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

Synthesis,structural study,thermal, optical properties and characterization of the new compound [C_6H_7N_2O_2]_3TeCl_5·2Cl

The new organic-inorganic compound, [C_6H_7N_2O_2]_3TeCl_5·2Cl was synthesized and its structure was determined at room temperature in the triclinic system (P~-1) with the following parameters: a = 10.5330(11) ?, b = 10.6663(11) ?, c = 15.9751(16)?, α = 82.090(2)°, β = 71.193(2)°, γ = 68.284(2)°and Z = 2. The final cycle of refinement led to R = 0.057 and Rw = 0.149. The crystal structure was stabilized by an extensive network of N--H···Cl and non-classical C--H···Cl hydrogen bonds between the cation and the anionic group. Several thermal analysis techniques such as thermogravimetric analysis, differential scanning calorimetric analysis and evolved gas analysis were used. We used isoconversional kinetics methods to determine the kinetics parameters. We observe that the decomposition of [C_6H_7N_2O_2]_3TeCl_5·2Cl entails the formation hydrochloric acid of nitroaniline as volatiles. The infrared spectra were recorded in the4000–400 cm~(-1)frequency region. The Raman spectra were recorded in the external region of the anionic sublattice vibration 50–1500 cm~(-1). The optical band gap was calculated from the UV-Vis absorbance spectra using classical Tauc relation which was found to be 3.12 and 3.67 eV.     

Synthesis, Structure and Characterization of Bis(ethylene-1,2-dithiolate)(μ_2-di-2-pyridyl-ketone p-phenyldiamine-N,N'''')-tin(IV) Dichloromethane

1 INTRODUCTION Sn(edt)2:[Sn(edt)2L]?CH2Cl2 through a one-pot reac- tion of Sn(edt)2, bis(2-pyridyl)ketone and p-phenyl- In recent years, the researches on tin sulfide mate- diamine in CH2Cl2. Herein we report the synthesis, rials draw increasing attention of chemists owning to crystal structure and characterization of the title com- their potential applications as photovoltaic materials, pound. holographic recording system[1, , solar control devi- 2] ces[3 and semiconductor materials. …     

Synthesis and Crystal Structure of [(NH_4)_6][Gd_2Mo_(36)O_(112)(H_2O)_(20)]·52H_2O

1 INTRODUCTION There is considerable interest in the heteropolymetalates in view of their potential applications in many fields, such as, catalysis, biology, medicine, magnetochemistry, and materials science[1～5]. It has been well- known that the rare earth elements are highly oxophilic and the anion of polyoxomolybdates have oxygen-rich composition, which can be used as synthons for the construction of novel heteropolymetalates. Since the structure of polyoxoanion 36-molybdate Mo36O1128…     

Crystal Structure and Interaction with DNA of [Ni(phen)(mal)(H_2O)_2]·3H_2O

1 INTRODUCTION In the last few years, much attention has been paid to the molecular structure and biological activity of coordinated complexes in inorganic chemistry field. Ni(Ⅱ) is one of the commonest transition metals with two coordination numbers (4 and 6)[1～3]. Ge- nerally speaking, Ni(Ⅱ) coordination mode depends on the structure of ligand, solvent and reaction con- ditions, among which ligand plays a decisive role and determines not only the molecular structure of the complex bu…     

Synthesis, Crystal Structure and Luminescent Properties of TbCu（TeO3）2Cl

TbCu(TeO3)2Cl was obtained in high yield from high temperature solid-state reac-ion of Tb4O7,CuO,CuCl2 and TeO2 in a 1:2:2:8 molar ratio at 710 ℃ in an evacuated quartz tube. Its structure was established by single-crystal X-ray diffraction. The title compound crystal-lizes in monoclinic,space group P21/c,with a=5.409(2),b=14.994(6),c=9.183(4),β= 98.884(5)°,V=735.8(5) ?3 and Z=4. TbCu(TeO3)2Cl is isostructural with LnCu(TeO3)2X (Ln= Dy,X= Cl; Ln=Er,X=Cl,Br). Its structure features a three-dimensional (3D) network built from Tb(Ⅲ) and Cu(II) ions interconnected by tellurite and chloride anions; the chloride anion and the lone-pair electrons of the tellurium(IV) ions are oriented toward the cavities of the tunnels in the network. Solid-state luminescent spectrum of TbCu(TeO3)2Cl shows a strong emission band at 545 nm with a luminescent life time of 291 μs.     

Synthesis and Structural Characterization of [(C_2H_5)_4N][V~((V))O_2(OC_6H_3(OCH_3)CHNNCSNH_2)]·H_2O

1 INTRODUCTIONAlthough vanadium plays an increasingly recognized role as a biometal[1~4], little is known about the structure and function of vanadium compounds in living organisms. A classical and nevertheless rapidly developing field of application for oxovanadates and related compounds is their use as catalysts in polymerization and oxidation reactions[5,6], and recent interest has focused on oxovanadates as model compounds for the interaction of oxovanadates with the active sites of en…     

Syntheses, Crystal Structures and Photoluminescence Properties of Cadmium(Ⅱ) and Nickel(Ⅱ) Complexes with 2-(2-Benzimidazolyl)quinoline

Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.     

Synthesis,Crystal Structure and Photoluminescence of [Gd(C_6NO_2H_5)_3-(H_2O)_2]_(2n)·(nH_5O_2)(nHgCl_5)(2nHgCl_4)·(2nH_2O)

A heterometallic 4f-5d inorganic-organic metal-isonicotinato hybrid Gd(C6NO2H5)3-(H2O)22n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydrothermal reaction and structurally characterized.Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell:a=24.234(8)=b=20.816(7)=c=15.333(3)=β=128.091(8)°=V=6088(3)3=C36H47Cl13Gd2Hg3N6O20=Mr=2260.92=Dc=2.467 g/cm3=S=0.896=μ(MoKα)=10.331 mm-1=F(000)=4216=R=0.0344 and wR=0.0629.The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure.Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.     

Synthesis and structural characterization of a novel dimolybdenum(Ⅰ) compound with mixed-tribridging ligands:[Bu_4N][Mo_2(μ-SPh)_2(μ-Cl)(CO)_6]

A novel mixed-trib ridged dimolybdenum(Ⅰ) compound [Bu4N][Mo2(n-SPh)2(u-Cl)(CO)6] (1) has been synthesized from the reaction of Mo2 (CO)8 (SPh)2 with ButNCl.Compound 1 was characterized by IR,UV-Vis and 1H,13C,95Mo NMR spectroscopic analyses.The electrochemical behavior was measured by cyclic voltammetry,indicating a quasi-reversible two-electron transfer in one step.The crystal structure determined by X-ray crystallography shows that 1 contains a [Mo2(u-S)2(u-Cl)]- core with a planar Mo2S2 unit and a Cl bridge.The Mo-Mo distance is 0.28709(7) nm,and the Mo-Cl-Mo angle is 66.44(4).A newface-sharing bioctahedral structure is discussed.     

Layered Lanthanum Complex with 3-Nitrophthalic Acid Assembled via Hydrogen Bonds-Synthesis, Structure and Characterization of [LaL(HL)(H_2O)_3]_2·2H_2O (H_2L=3-NO_2C_6H_3(CO_2H)_2)

A new dinuclear centrosymmetric complex [LaL(HL)(H2O)3]2·2H2O (H2L = 3-nitro- phthalic acid, NPA) was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1 with a = 8.1549(16), b = 8.8856(18), c = 15.277(3) , α = 100.93(3), β = 90.81(3), γ = 104.56(3)°, V = 1049.8(4) 3, Z = 1, μ = 2.125 mm-1, Dc = 1.994 g/cm3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates(2-) coordinate with the La3+ ions in a bridging mode, and two monohydrogen- 3-nitrophthates(1-) and three waters in terminal ways, respectively. Each La3+ ion is nine- coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C–H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.     

Hydrothermal Synthesis, Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH2]2+·[SbCl5]2-}2

A new supramolecular compound, {[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetric analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 16.0397(13), b = 14.3189(12), c = 15.6370(13) (A), β = 105.8980(10)°, V = 3454.0(5) (A)3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3, μ = 2.366 mm-1, S = 1.010, F(000) = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb…C1.Moreover,the compund adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridy1)benzimidazole divalent cations.The title compound also shows godd fluorescent behaviors.     

Synthesis and Structure Study of Molybdenum Complex Mo[o-NHCOCH_3-m-NO_2C_6H_3COOH]_2_O2Cl_2·PhCl

The crystal and molecular structures of molybdenum complex, Mo [ o- NHCOCH3- m-NO2C6H3COOH]2O2Cl2.PhCl are reported. The crystal belongs to space group Cc of monoclinic system with unit cell parameters:α= 11. 214 (3) A .b= 19. 544 (4 ) A . c = 14. 091 (6) A .β=94.06(3)°,V'=3080.3 A3 and Z=4. The structure was refined to R=0. 061.The coordination number for the Mo atom Is six. The coordination polyhedron formed by four O atoms and two Cl atoms around the Mo atom is a distorted octahedron. Four O atoms and one Mo atom construct a plane. Two benzyl planes in coordinate groups and the benzyl plane of solvent are almost parallel. The quantum-chemical calculations were carried out. There are hydrogen bonds in the Complex. The EHMO calculations and the existence of hydrogen bonds prove that the O atoms are stronger coordinated atoms in the carbonyls than in the carboxyls.     

Preparation and Molecular Structure of (SCZ)(TNPG)·2H_2O

1 INTRODUCTION 2,4,6-Trinitro-1,3,5-trihydroxybenzene(trinitro- phloroglucinol, TNPG) is a strong acidic organic com- pound with yellow needle crystal structure. There are three nitro-groups and three phenolic hydroxyl groups conjugated with the ring, so it is an important explosive. It can react with metallic compounds forming metallic salts of TNPG, which have strong combustion and detonating properties. The lead salt of TNPG has been extensively studied and recom- mended to use as…     

THEORETICAL STUDIES ON CARBENES AND CARBENOIDS (Ⅳ) ——ISOMERIZATIONS AND DECOMPOSITIONS OF CARBENOIDS H_2C=CLiCl AND H_2CLiCl

The isomerizations and decompositions of carbenoids H_2C=CLiCl and H_2CLiCl have been studied by use of HF/STO-3G gradient method. Three equilibrium structures of H_2C=CLiCl were obtained, in which the linear structure has the lowest energy and the askew substituted structure was the next. It is found that the decomposition of H_2C=CLiCl undergoes a concerted FBW rearrangement and the inversion barrier of its askew substituted structure is 36 kJ/mol. For H_2CLiCl, the askew substituted structure, extending all valences of the carbon into a single hemisphere, is the lowest energy and its inversion barrier is 87 kJ/mol. The discussions on the factors concerned with the structural stabilities are given in this paper.     

STRUCTURE OF PENTAAQUO PYROMEL DIZINE (Ⅱ)-DIHYDROUS [C_6H_2(COO)_4Zn_2(H_2O)_5]·2H_2O

Crystal and molecular structure of [C6H2(COO)4Zn2(H2O)5]·2H2O has been determined by X-ray diffraction technique, Mr = 507. 0,monoclinic,space group P21/n,a = 5. 925(1), 6 = 23. 613(9) ,c= 11. 790(5) A ,β= 96. 36 (3)°, V=1639. 3 (1. 0) A3,Z=4,DC = 2. 05g/cm3,λ=0. 71069 A,μ(MoKa) = 30. 9/cm-1,F(000) = 1024e. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0. 055(Re = 0. 059)for 1557(I>3σ(I))reflections. Both atoms Zn(1) and Zn(2) are bridged by the Z,E-type of the car-boxyl group, in addition, Zn (1) is monodentate-bonded to the three remaining carboxyl and Zn(2) is bonded to five water molecules. The crystal structure shows a 2-dimensional polymeric network along(010)face. The Zn(l) -O distances are in the range of 1. 94~ 2. 01 A (average 1. 98 A ). The Zn(2) -O distances are in the range of 2. 06~2. 21 A (average 2. 12A).     

Hydrothermal Synthesis and Structure of a Novel Coordination Polymer Co_3(tma)(pda)_2(H_2O)_3]n·nH_2O

1INTRODUCTION Recently,the design and preparation of coordina-tion polymers with new porous frameworks are of great interest due to their potential functionalities such as catalysis,gas absorption,separation and molecu-lar recognition.In designing1-D,2-D and3-D porous coordination polymers,the selection of appropriate ligands is crucial for determining the structure.The mixed-linker systems of both carboxylates and pyri-dyls have proved to be effective for the preparation of novel coordi…